CN101857211A - Method for preparing industrial grade monoammonium phosphate from wet-process phosphoric acid - Google Patents
Method for preparing industrial grade monoammonium phosphate from wet-process phosphoric acid Download PDFInfo
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- CN101857211A CN101857211A CN201010191938A CN201010191938A CN101857211A CN 101857211 A CN101857211 A CN 101857211A CN 201010191938 A CN201010191938 A CN 201010191938A CN 201010191938 A CN201010191938 A CN 201010191938A CN 101857211 A CN101857211 A CN 101857211A
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Abstract
The invention discloses a method for preparing industrial grade monoammonium phosphate from wet-process phosphoric acid. In the method, the industrial grade monoammonium phosphate is prepared by neutralizing ammonia with low-cost wet-process phosphoric acid serving as raw materials; a pickling procedure is adopted, so that volatile gas materials are recycled, crystallization mother liquor is recycled or concentrated for recycling, the industrial grade monoammonium phosphate product is obtained, and the product yield is improved; meanwhile the by-products in the production process are used as compound fertilizer materials. The method has the advantages of greatly reducing the production cost of the industrial grade monoammonium phosphate, guaranteeing the stability of the product quality, and avoiding secondary pollution, along with low energy consumption and better economic benefit and social benefit.
Description
Technical field:
The invention belongs to the phosphorus chemical product preparing technical field, relate to a kind of method with preparing industrial grade monoammonium phosphate from wet-process phosphoric acid.
Background technology:
Monoammonium phosphate claims primary ammonium phosphate again, and molecular formula is NH
4H
2PO
4Monoammonium phosphate mainly is used as the fireproofing agent of timber, paper, fabric etc.
In prior art, manufacture level monoammonium phosphate adopts traditional method more, promptly utilizes the direct neutralization reaction of thermal phosphoric acid and ammonia to generate.Though production process equipment is simple, the quality product height, apparatus and process technical requirements height, cost is big, the energy consumption height.At present, adopt the technology of Wet-process Phosphoric Acid Production monoammonium phosphate to be favored by people.Proposed a kind of method as Chinese patent 85103677.5, used the phosphoric acid by wet process and the ammonia neutralization of higher concentration and form phosphoric acid one ammonium crystalline slip, obtained industrial grade monoammonium phosphate after separating after filtration with Wet-process Phosphoric Acid Production pure phosphoric acid one ammonium.Though this method technical process is shorter, product purity is not high, and energy consumption is big, the operational requirement height, and the phosphorus total yield is low.Chinese patent 92108090.5 has proposed a kind of production method of industrial grade monoammonium phosphate, in phosphoric acid by wet process and the ammonia and after, through natural subsidence, the slurry that obtains is in order to preparation fertilizer grade monoammonium phosphate, and clear liquid obtains the industrial grade monoammonium phosphate product through crystallization, separation, washing, drying.Though this method is simple to operate, quality product is better, because of adopting the method for natural subsidence to separate clear liquid and slurry with the back in phosphoric acid by wet process and the ammonia, the production cycle is longer, and overall benefit is not high.Chinese patent 200810196872.4 has proposed a kind of technology of usefulness phosphoric acid by wet process continuous production industrial grade monoammonium phosphate, and phosphoric acid by wet process passes through in the secondary and secondary filtration, and filtrate makes industrial grade monoammonium phosphate through the evaporative crystallization drying.Though this method can obtain the quality high product, technical process is longer, and trivial operations is not enough desirable.
Summary of the invention:
Purpose of the present invention: in order to overcome the problem that prior art exists, guarantee that whole process of production avoids secondary pollution and cut down the consumption of energy, improve the product yield, make it have favorable economic benefit and social benefit, a kind of method with preparing industrial grade monoammonium phosphate from wet-process phosphoric acid is provided.
Technical scheme of the present invention is:
Adopt cheaply that phosphoric acid by wet process and ammonia are raw material, carry out neutralization reaction, strict CONTROL PROCESS condition, guarantee the stability of quality product, crystalline mother solution reclaims and uses, and adopts pickling process that the evaporable ammonia is reclaimed simultaneously and uses, cut down the consumption of raw materials, and avoid secondary pollution.
The present invention is achieved in that
With the method for preparing industrial grade monoammonium phosphate from wet-process phosphoric acid, be to be raw material with the phosphoric acid by wet process, make with the ammonia neutralization reaction, comprising: neutralization, filtration, pickling, concentrate, crystallization, centrifugal and drying process, the concrete operations step is as follows:
A. drop into the crystalline mother solution that reactor volume 5～20% loops back in reactor, start agitator, slowly adding weight concentration in mother liquor then is 38～42%P
2O
5Phosphoric acid by wet process, and slowly feed ammonia, neutralization reaction is carried out in control PH=4.4～4.6 under 30～100 ℃ of temperature, after absorbing the evaporable ammonia, pickling process is back in the reactor simultaneously, control PH=4.4～4.6 are the neutralization reaction terminal point, after stopping to feed intake, continue to stir 10～90 minutes, obtain the industrial grade monoammonium phosphate slip;
B. the industrial grade monoammonium phosphate slip that a step is obtained carries out solid-liquid separation, removes impurity, and filter cake is sent to composite fertilizer source mill;
C. the industrial grade monoammonium phosphate solution that the b step is obtained is delivered to heat in the concentrating unit and is concentrated, and till having micro-crystallization to occur, the evaporable ammonia returns in the reactor after pickling process absorbs;
D. the concentrated solution with the c step moves in the crystallizer tank, at temperature crystallisation by cooling below 40 ℃, forms the industrial grade monoammonium phosphate xln;
E. with the industrial grade monoammonium phosphate xln of d step, carry out the solid-liquid separation second time, mother liquor returns a or c step, and xln makes industrial grade monoammonium phosphate after super-dry.
Above-described reactor equipment comprises stainless steel cauldron, inner liner polytetrafluoroethylene reactor and enamel reaction still.
The equipment that above-described pickling is adopted comprises bubble absorbing tower, packed absorber and tray absorption columns.
The equipment of above-described concentrated employing is vacuum concentrator.
The equipment that above-described solid-liquid separation adopts, solid-liquid separation adopts plate-and-frame filter press for the first time, and solid-liquid separation adopts whizzer for the second time.
The above-described dry equipment that adopts comprises rotating drum dryer and vibratory screening apparatus drying machine.
The connection of above-described equipment, comprise reactor respectively with being connected of plate-and-frame filter press and absorption tower, vacuum concentrator respectively with being connected of plate-and-frame filter press, absorption tower and crystallizer tank, crystallizer tank is connected with whizzer, whizzer is connected with moisture eliminator.
Advantage of the present invention and positively effect:
1. be raw material with the phosphoric acid by wet process, reclaim crystalline mother solution and volatilization raw material, improve the product yield, greatly reduce production cost;
2. strict CONTROL PROCESS condition, quality product height, good stability;
3. the byproduct in the production process can be made composite fertilizer's raw material, and the volatilization raw material reclaims and uses, and Recycling Mother Solution is used, and avoids secondary pollution, has both protected environment, reduces the three wastes and energy consumption again, has favorable economic benefit and social benefit.
Description of drawings:
Accompanying drawing 1: be process flow diagram of the present invention.
As shown in the figure, technical process of the present invention mainly comprises: neutralization, filtration, pickling, evaporation, crystallization, centrifugal and drying process.
Embodiment:
The invention will be further described below in conjunction with accompanying drawing with by embodiment, and listed embodiment only is the present invention is described and never is limited to the present invention.
Embodiment one
In enamel reaction still, drop into the recovery crystalline mother solution of reactor volume 20%, start agitator, slowly in mother liquor, add weight concentration 40%P then
2O
5Phosphoric acid by wet process, and slowly feed ammonia, control PH=4.4 carries out neutralization reaction under 55 ℃ of temperature, the evaporable ammonia is back in the reactor after the pickling bubble absorbing tower absorbs, control PH=4.4 is the neutralization reaction terminal point, after stopping to feed intake, continue to stir 20 minutes, obtain the industrial grade monoammonium phosphate slip; With the industrial grade monoammonium phosphate slip plate-and-frame filter press filtered while hot that obtains, remove impurity, filter cake is sent to composite fertilizer source mill; The industrial grade monoammonium phosphate solution that obtains is delivered to the vacuum concentrator heating concentrate, crystalline film occurs until the surface, the pickling bubble absorbing tower is back to reaction kettle for reaction after the evaporable ammonia is absorbed; Concentrated solution is moved in the crystallizer tank, form the industrial grade monoammonium phosphate xln at 40 ℃ of following crystallisation by cooling of temperature, then carry out centrifugation with whizzer, recycle or the concentrated industrial grade monoammonium phosphate product that reclaims of warp with operation during mother liquor returns, make industrial grade monoammonium phosphate after the xln process rotating drum dryer drying.
Embodiment two
In stainless steel cauldron, drop into the recovery crystalline mother solution of reactor volume 15%, start agitator, slowly in mother liquor, add weight concentration 38%P then
2O
5Phosphoric acid by wet process, and slowly feed ammonia, control PH=4.6 carries out neutralization reaction under 70 ℃ of temperature, the evaporable ammonia is back in the reactor after the pickling packed absorber absorbs, control PH=4.6 is the neutralization reaction terminal point, after stopping to feed intake, continue to stir 30 minutes, obtain the industrial grade monoammonium phosphate slip; With the industrial grade monoammonium phosphate slip plate-and-frame filter press filtered while hot that obtains, remove impurity, filter cake is sent to composite fertilizer source mill; To obtain industrial grade monoammonium phosphate solution and deliver to vacuum concentrator heating and concentrate, and crystalline film occur until the surface, the pickling packed absorber is back to reaction kettle for reaction after the evaporable ammonia is absorbed; Concentrated solution is moved in the crystallizer tank, form the industrial grade monoammonium phosphate xln at 35 ℃ of following crystallisation by cooling of temperature, then carry out centrifugation with whizzer, recycle or the concentrated industrial grade monoammonium phosphate product that reclaims of warp with operation during mother liquor returns, make industrial grade monoammonium phosphate after the xln process vibratory screening apparatus drying machine drying.
Claims (7)
1. the method with preparing industrial grade monoammonium phosphate from wet-process phosphoric acid is to be raw material with the phosphoric acid by wet process, makes with the ammonia neutralization reaction, it is characterized in that: comprise neutralization, filtration, concentrate, pickling, crystallization, centrifugal and drying process that the concrete operations step is as follows:
A. drop into the crystalline mother solution that reactor volume 5～20% loops back in reactor, start agitator, slowly adding weight concentration in mother liquor then is 38～42%P
2O
5Phosphoric acid by wet process, and slowly feed ammonia, neutralization reaction is carried out in control PH=4.4～4.6 under 30～100 ℃ of temperature, after absorbing the evaporable ammonia, pickling process is back in the reactor simultaneously, control PH=4.4～4.6 are the neutralization reaction terminal point, after stopping to feed intake, continue to stir 10～90 minutes, obtain the industrial grade monoammonium phosphate slip;
B. the industrial grade monoammonium phosphate slip that a step is obtained carries out solid-liquid separation, removes impurity, and filter cake is sent to composite fertilizer source mill;
C. the industrial grade monoammonium phosphate solution that the b step is obtained is delivered to heat in the concentrating unit and is concentrated, and till having micro-crystallization to occur, the evaporable ammonia returns in the reactor after pickling process absorbs;
D. the concentrated solution with the c step moves in the crystallizer tank, at temperature crystallisation by cooling below 40 ℃, forms the industrial grade monoammonium phosphate xln;
E. with the industrial grade monoammonium phosphate xln of d step, carry out the solid-liquid separation second time, mother liquor returns a or c step, and xln makes industrial grade monoammonium phosphate after super-dry.
2. the method with preparing industrial grade monoammonium phosphate from wet-process phosphoric acid according to claim 1, it is characterized in that: reactor equipment comprises stainless steel cauldron, inner liner polytetrafluoroethylene reactor and enamel reaction still.
3. the method with preparing industrial grade monoammonium phosphate from wet-process phosphoric acid according to claim 1, it is characterized in that: absorption equipment comprises bubble absorbing tower, packed absorber and tray absorption columns.
4. the method with preparing industrial grade monoammonium phosphate from wet-process phosphoric acid according to claim 1, it is characterized in that: thickening equipment is a vacuum concentrator.
5. the method with preparing industrial grade monoammonium phosphate from wet-process phosphoric acid according to claim 1 is characterized in that: the plate-and-frame filter press of solid-liquid separation employing for the first time in the solid-liquid separating equipment, separate for the second time and adopt whizzer.
6. the method with preparing industrial grade monoammonium phosphate from wet-process phosphoric acid according to claim 1, it is characterized in that: drying plant comprises rotating drum dryer and vibratory screening apparatus drying machine.
7. the method with preparing industrial grade monoammonium phosphate from wet-process phosphoric acid according to claim 1, it is characterized in that: the mode of connection of equipment is: reactor respectively with being connected of plate-and-frame filter press and absorption tower, vacuum concentrator respectively with being connected of plate-and-frame filter press, absorption tower and crystallizer tank, crystallizer tank is connected with whizzer, and whizzer is connected with moisture eliminator.
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| CN201010191938A CN101857211A (en) | 2010-06-04 | 2010-06-04 | Method for preparing industrial grade monoammonium phosphate from wet-process phosphoric acid |
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| CN201010191938A CN101857211A (en) | 2010-06-04 | 2010-06-04 | Method for preparing industrial grade monoammonium phosphate from wet-process phosphoric acid |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102320585A (en) * | 2011-09-01 | 2012-01-18 | 贵州开磷（集团）有限责任公司 | Method for direct production of industrial-grade ammonium biphosphate by wet-process phosphoric acid |
| CN102976869A (en) * | 2012-12-06 | 2013-03-20 | 江苏湛蓝科技开发有限公司 | Technique for producing macroelement water-soluble fertilizer and coproducing slow-release fertilizer |
| CN103569982A (en) * | 2013-11-08 | 2014-02-12 | 武汉工程大学 | Method for crystallizing large-grained industrial ammonium dihydrogen phosphate |
| CN104072208A (en) * | 2014-07-16 | 2014-10-01 | 云南常青树化工有限公司 | Preparation method for water soluble fertilizer |
| CN104340963A (en) * | 2013-07-23 | 2015-02-11 | 耿兆翔 | Efficient ammonium biphosphate production method |
| CN104528675A (en) * | 2015-01-30 | 2015-04-22 | 达州瓮福蓝剑化工有限责任公司 | Method and stirring device for producing crystalline monoammonium phosphate by using wet-process purified phosphoric acid |
| CN104860282A (en) * | 2015-04-17 | 2015-08-26 | 湖北六国化工股份有限公司 | Method for recovering condensation waste liquid in industrial monoammonium phosphate device |
| CN105130549A (en) * | 2015-07-14 | 2015-12-09 | 湖北三宁化工股份有限公司 | Method of producing macro-element water-soluble fertilizer from industrial-grade monoammonium phosphate mother liquid |
| CN107746291A (en) * | 2017-10-24 | 2018-03-02 | 贵州大学 | A kind of method of MAP anti-caking |
| CN109279590A (en) * | 2018-11-22 | 2019-01-29 | 嘉兴市环科环保新材料科技有限公司 | A kind of waste phosphoric acid generates the process of ammonium dihydrogen phosphate |
| CN110681487A (en) * | 2019-09-27 | 2020-01-14 | 瓮福达州化工有限责任公司 | Iron removing system and preparation process thereof |
| CN110937585A (en) * | 2019-12-16 | 2020-03-31 | 瓮福达州化工有限责任公司 | Production method of industrial-grade monoammonium phosphate |
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| US3563723A (en) * | 1969-04-02 | 1971-02-16 | Sackett & Sons Co A J | Method and system for manufacturing ammonium phosphates |
| EP0161704A2 (en) * | 1984-04-18 | 1985-11-21 | ENICHEM AGRICOLTURA S.p.A. | Process for the production of water soluble ammonium phosphates |
| CN1305945A (en) * | 2001-02-28 | 2001-08-01 | 四川龙蟒集团有限责任公司 | Process for preparing feed-class, industry-class, or technical-class monoammonium phosphate |
| CN101367512A (en) * | 2008-09-05 | 2009-02-18 | 湖北祥云(集团)化工股份有限公司 | Process for continuous production of technical grade mano-ammonium phosphate with wet-process and phosphoric acid |
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2010
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US3563723A (en) * | 1969-04-02 | 1971-02-16 | Sackett & Sons Co A J | Method and system for manufacturing ammonium phosphates |
| EP0161704A2 (en) * | 1984-04-18 | 1985-11-21 | ENICHEM AGRICOLTURA S.p.A. | Process for the production of water soluble ammonium phosphates |
| CN1305945A (en) * | 2001-02-28 | 2001-08-01 | 四川龙蟒集团有限责任公司 | Process for preparing feed-class, industry-class, or technical-class monoammonium phosphate |
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102320585B (en) * | 2011-09-01 | 2014-07-02 | 贵阳中化开磷化肥有限公司 | Method for direct production of industrial-grade ammonium biphosphate by wet-process phosphoric acid |
| CN102320585A (en) * | 2011-09-01 | 2012-01-18 | 贵州开磷（集团）有限责任公司 | Method for direct production of industrial-grade ammonium biphosphate by wet-process phosphoric acid |
| CN102976869A (en) * | 2012-12-06 | 2013-03-20 | 江苏湛蓝科技开发有限公司 | Technique for producing macroelement water-soluble fertilizer and coproducing slow-release fertilizer |
| CN104340963A (en) * | 2013-07-23 | 2015-02-11 | 耿兆翔 | Efficient ammonium biphosphate production method |
| CN103569982A (en) * | 2013-11-08 | 2014-02-12 | 武汉工程大学 | Method for crystallizing large-grained industrial ammonium dihydrogen phosphate |
| CN103569982B (en) * | 2013-11-08 | 2015-05-20 | 武汉工程大学 | Method for crystallizing large-grained industrial ammonium dihydrogen phosphate |
| CN104072208A (en) * | 2014-07-16 | 2014-10-01 | 云南常青树化工有限公司 | Preparation method for water soluble fertilizer |
| CN104528675B (en) * | 2015-01-30 | 2016-06-01 | 达州瓮福蓝剑化工有限责任公司 | Utilize method and the whipping appts of wet purification phosphoric acid production crystal phosphoric acid one ammonium |
| CN104528675A (en) * | 2015-01-30 | 2015-04-22 | 达州瓮福蓝剑化工有限责任公司 | Method and stirring device for producing crystalline monoammonium phosphate by using wet-process purified phosphoric acid |
| CN104860282A (en) * | 2015-04-17 | 2015-08-26 | 湖北六国化工股份有限公司 | Method for recovering condensation waste liquid in industrial monoammonium phosphate device |
| CN104860282B (en) * | 2015-04-17 | 2016-03-02 | 湖北六国化工股份有限公司 | A kind of method reclaiming condensation waste liquid in industrial grade monoammonium phosphate device |
| CN105130549A (en) * | 2015-07-14 | 2015-12-09 | 湖北三宁化工股份有限公司 | Method of producing macro-element water-soluble fertilizer from industrial-grade monoammonium phosphate mother liquid |
| CN107746291A (en) * | 2017-10-24 | 2018-03-02 | 贵州大学 | A kind of method of MAP anti-caking |
| CN109279590A (en) * | 2018-11-22 | 2019-01-29 | 嘉兴市环科环保新材料科技有限公司 | A kind of waste phosphoric acid generates the process of ammonium dihydrogen phosphate |
| CN110681487A (en) * | 2019-09-27 | 2020-01-14 | 瓮福达州化工有限责任公司 | Iron removing system and preparation process thereof |
| CN110937585A (en) * | 2019-12-16 | 2020-03-31 | 瓮福达州化工有限责任公司 | Production method of industrial-grade monoammonium phosphate |
| CN110937585B (en) * | 2019-12-16 | 2023-03-10 | 瓮福达州化工有限责任公司 | Production method of industrial-grade monoammonium phosphate |
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